Furlanetto S, Pinzauti S, Gratteri P, La Porta E, Calzeroni G
Dipartimento di Scienze Farmaceutiche, Università di Firenze, Florence, Italy.
J Pharm Biomed Anal. 1997 Jun;15(9-10):1585-94. doi: 10.1016/s0731-7085(96)02029-8.
Experimental design was used for the optimization and robustness testing of an adsorptive stripping voltammetric procedure for kynurenic acid determination. The optimization of the peak height response proceeded through a screening phase (D-optimal design strategy) followed by a response surface study (Doehlert design) applied to the variables pH, pulse amplitude and stirring rate. An interaction between pH and stirring rate was pointed out. The optimized method was validated and the variation of factors that was expected to occur in practice was simulated in a robustness test. A composite fractional matrix for the evaluation of method robustness was used and pH emerged as the only critical factor. The linear range found applying the optimized conditions was 2.5 x 10(-9) to 2.5 x 10(-7) M and the calculated limit of detection was 1.72 x 10(-9) M.
采用实验设计对用于犬尿喹啉酸测定的吸附溶出伏安法进行优化和稳健性测试。通过筛选阶段（D - 最优设计策略），随后对变量pH、脉冲幅度和搅拌速率进行响应面研究（Doehlert设计），来优化峰高响应。指出了pH和搅拌速率之间的相互作用。对优化后的方法进行了验证，并在稳健性测试中模拟了实际中可能出现的因素变化。使用了一个复合分数矩阵来评估方法的稳健性，结果表明pH是唯一的关键因素。在优化条件下得到的线性范围为2.5×10⁻⁹至2.5×10⁻⁷ M，计算出的检测限为1.72×10⁻⁹ M。
